Patent GB-510165-A (GB)
Title: Improvements in or relating to the manufacture of cellulose
IPC: D21B1/00
Filed: 1938-01-27
Abstract: 510,165. Refining cellulosic materials. DREYFUS, H. Jan. 27, 1938, No. 2617. [Class 2 (ii)] Cellulose is manufactured by impregnating lignin-containing cellulosic materials, for instance wood in the form of chips, sawdust or mechanical pulp, with dilute nitric acid under conditions such that the lignin is substantially unattacked, concentrating the acid in contact with the materials and thereafter subjecting the materials containing the thus concentrated acid to a temperature at which the nitric acid attacks the lignin contained therein. The cellulosic raw materials may be subjected to various preliminary treatments to facilitate their thorough impregnation with the nitric acid. Thus, they may be subjected to a preliminary boil with water, a dilute alkali such as caustic soda, or a dilute acid, or any air in the materials may be preliminarily replaced by steam, or the materials may be heated with water under considerable pressure and the pressure suddenly released, or the vessel containing the materials may be evacuated before introducing the nitric acid. Alternatively, the nitric acid may be forced into the materials under pressure. The. concentration of the nitric acid may be effected under reduced pressure and aided by passing a stream of warm or cold air, nitrogen or other gas over or through the materials. If desired, a substance, such as benzene, forming with water a constant boiling mixture of boiling point lower than 100‹C. may be added to the dilute acid to assist in the concentration. Following the treatment with nitric acid, the cellulose may be washed with water or a dilute solution of an alkali such as caustic soda and may then be subjected to a one or two stage treatment with alkali, for example first with dilute alkali at elevated temperature and then with cold, more concentrated alkali. The cellulose produced may be bleached, for example, with chlorine or hypochlorite, and is suitable for the manufacture of paper, viscose and cellulose esters and ethers. Where the cellulose is to be used in the manufacture of organic esters of cellulose, it may be activated by treatment with a lower fatty acid and/or a mineral acid in liquid or vapour form. In an example, spruce chips are boiled for one hour with water or 2 per cent. caustic soda solution and then washed with water. They are then immersed at room temperature in eight times their weight of 2¢ per cent. nitric acid for eight hours. The temperature is then raised to 35-40‹C. and the pressure in the vessel reduced until water is being rapidly evaporated from the dilute acid, a stream of air heated to about 60‹C. is blown through the vessel under the reduced pressure until the acid remaining has a concentration of about 20 per cent. The materials are then allowed to stand at atmospheric pressure and at about 50‹C. for a few hours. The product is washed with hot water, boiled with 4 per cent. caustic soda solution under about 8 atmospheres pressure, washed and allowed to stand 2-3 hours in 10 per cent. caustic soda solution at room temperature. The product, after a further washing, may be bleached first with chlorine and then with an alkaline hypochlorite solution. Specifications 263,938 and 312,098, [both in Class 2 (ii)], and French Specification 565,654 are referred to.